IS 11720 (Part 6): 2001

mi9n7m

(Reaffirmed - 2012)

mmz GF@tm Tmfwrr
W16fklIW%W@l~?KIT

Indian Standard

METHODS OF TEST FOR SYNTHETIC RUBBER
PART 6 DETERMINATION OF SOLVENT EXTRACT

ICS 71.040.4083.060

BUREAU
MANAK

OF

INDIAN

STANDARDS
ZAFAR MARG

BHAVAN, 9 BAHADUR SHAH NEW DELHI 11O(K)2

Ocrober2001

Price Group 3

Rubber Sectional Committee. PCD 14

FOREWORD This Indian Standard (Part 6) was adopted by the Bureau of Indian Standards, after the draft finalized by the Rubber Sectional Committee had been approved by the Petroleum, Coal and Related Products Division Council. The concerned Committee has decided to prepare common methods of test for synthetic rubber under SR (Synthetic Rubber) series, namely, IS 11720 and this will be applicable to rdl types of synthetic rubbers being produced indigenously. This standard (part 6) is the sixth in the series. The other standards of this series are as follows: Part 1 Part 2 Part 3 Part 4 Part 5 Methods of test for synthetic rubber: Part 1 Determination of antioxidant (SR 1) Methods of test for synthetic rubbem Part 2 Measurement of vulcanization characteristics with oscillating disc curemeter (SR2) Methods of test for synthetic rubbec Part 3 Determination of mooney viscosity Methods of test for synthetic rubber: Part 4 Determination of volatile matter Methods of test for synthetic rubbec Part 5 Determination of ash

Part 11 Methods of test for synthetic rubbe~ Part 11 Rubber raw styrene- butadiene -- Determination of soap and organic-acid content Part 13 Methods of test for synthetic rubber: Part 13 Determination of Gel content In the preparation of this standard, considerable assistance has been derived from ISO/DIS 1407 Rubber -- Determination of solvent extract issued by the International Organization for Standardization (1S0). The composition of the Committee responsible for formulation of this standard is given in Annex A. In reporting the results of a test or analysis made in accordance with this standard, if final value, observed or calculated is to be rounded off, it shall be done in accordance with IS 2:1960 `Rules for rounding off numerical values (revised)'.

ISl1720(Part6)

:2001

Indian Standard

METHODS OF TEST FOR SYNTHETIC RUBBER
PART 6 DETERMINATION
1 SCOPE 1.1 This Indian Standard (Part 6) prescribes the quantitative determination of total extractable materials from raw rubbers both natural and synthetic (SBR, CR, NBR, IR and IIR) and their unvulcanized and vulcanized compounds. 1.2 Two methods are adopted here: a) Method A is a rapid extraction method; and b) Method B is for use in case of dispute. 1.3 These methods are intended to determine the various organic constituents in the rubber like rosin, fatty acids, soaps extender oils, defoamer tars, antioxidants and other uncombined organic constituents which are extractable in the solvent used. The rubber hydrocarbon can also be estimated by subtracting the sum of the total extract, the total ash and the total volatile matter from 100. 2 REFERENCE The following Indian Standard contains provisions which, through tvferencein this tex~constituteprovisions of this standard. At the time of publication the edition indicated was valid. All standards are subject to revision, and parties to agreements based on the standard is encouraged to investigate the possibility of applying the most recent edition of the standard indicated below: IS No. 4518 (Part 1): 1967 litle Methods of test for styrenebutadiene rubbers (SBR): Part 1 Determination of volatile matter, total ash, organic acid, soap, antioxidants, bound styrene and moony viscosity

OF SOLVENT EXTRACT
Method A generally gives results which are lower than those obtained with Method B due to an equilibrium being set up particularly if large test portions are used. `lhble 1 Recommended Solvents (Clause 3.1) SI
No. (1) i) ii) (2) IR, NR SBR CR NBR HR Rubberl) Raw Rubbers and Unvulcanized Cornpounds (3) Acetonez) ETA Propan-2-ol Propan-2-ol Acetonez) Vulcanizates

iii)
iv) v)

(4) Acetone?) ETA Methanol Propan-2-ol Acetone2)

OIR . ]soprene Rubber, NR - Natural Rubber, SBR - StyreneButadiene Rubber, GR-ChIoroprene Rubber, NBR - Acrylonitrile Butadiene Rubber and IIR - Isobutene-Isoprene Rubber ~When acetone is used it may be partially boiling diacetone alcohol, If a difficult solvent is observed during the drying step, of diacetone, repeat the extraction using a use Method B. converted into high evaporation of the due to the presence different solvent or

4 REAGm WARNING: All recognized health and safety precautions should be taken when using the reagents. During the analysis, use only solvents recognized analytical grade. 4.1 Acetone 4.2 Ethanol toluene are azeotropic mixture (ETA), a mixture of 70 volumes of ethanol and 30 volumes of toluene. Reflex for 4 h over freshly calcined calcium oxide. Distill and collect a middle fraction with a boiling range of not more than lW. If absolute ethanol is used, the drying over calcium oxide may be omitted. 43 Proptm-2-ol(rso-propanol) 4A Methanol 5 APPARATUS 5.1 ExtractionApparatus The following three types of extraction apparatus are described. Any other type of apparatus which performs the same function may be used: a) The Type 1 apparatus comprises a receiver flask, jacketed soxhlet extractor and a condenser as shown in Fig. 1. 1

3 LIMI'E4TIONS 3.1 These methods are applicable to the rubbers given in Table 1. 3.2 The solvents recommended for individual rubbers are listed in Table 1, although other combinations may be desirable in certain cases. For instance, alcohols are particularly useful for extraction of vulcanized IR, NR and SBR where the extract will be used for thinlayer chromatography and not primarily for quantitative determination of amount of extractable. 3.3 The same quantitative results may not necessarily be obtained with either Method A or Method B not with the different solvents.

IS 11720(Part 6) :2001 b) The Type 2 apparatus comprises a 250 ml receiver flask, a condenser and an extraction cup suspended by clean wire as shown in Fig. 2. c) The~ 3 apparatus comprises a 250 ml receiver flask, a condenser and a Soxhlet extractor with a side arm as shown in Fig. 3. Typical Soxhlet capacityis lCKJrnlto200ml. Thexeisnoextraction cup.

A

JOINT B.
\&

r

JOINT A EXTRACTION

/ P
fi~pAclTv

RECEWERFLAW 250 cm3)

AU Dimensions in millimetres.
RECEIVER FLASK (CAPACITY 150 ems)

Fm. 3 Tm 3 ALL-GLASSEXTRACTION APPARATUS 5? Distillation head and condenser (not shown in the figures), appropriate for the apparatus to distill of the solvent after extraction. %3 Oven operatingat 100 *2%!. 5.4 Filterpaperor nylon filter cloth, extractedbefore use withthesame solventas thatusedfortheextraction. 53 Hot Plate 5.6 Sieve 150 Micrometer (100 Mesh)

FIG.1 TYPE1 ALL-GLASS EXTRACTION Amm,wws

\ UfF
/

5.7 Method for `IhkingOut Samples The method for taking out samples shall be in accordance with the method prescribed in3ofIS4518 (Part 1)for raw styrene-butadiene rubbers (SBR). Take a portion of the raw rubber at least 250 g collected as above and pass it through the cold rolls of a laboratory mill set to a nip not exceeding 0.5 mm. For vulcanizates, the analyst shall, by inspection, assure himself that the vulcanizates has not been contaminated. The sample to be analysed shall be selected by taking pieces for various parts of the original sample and separating them from foreign matter. For soil vulcanized rubber it is preferable to mix the sample and grind it by passing it two or three times through a clean, cold, laboratory rubber-mill. The rubber will come from the mill in the form of a coarse powder or a rough sheet. If the product 2

i------~M-lNT 2

HOOKS

RECEIVER FLASK (CAPACITY 254 cm3)

)

AH Dimensions in mi]limetres.

FIG.2 TYPE 2 ALL-GLASS EXTRACTION APPARATS

IS 11720(Part 6) :2001 is in the form of a sheet, the adjustment of the mill shall be such that the thickness of the final sheet is not greater than 0.5 mm. If the milled sample is a powder, it shall be transferred to a No. 14(1.40 micrometer) sieve and rubbed through the sieve. Grinding shall be continued until the entire sample passes through the sieve. In the absence of milling machinery, the sample may be prepared by cutting it with scissors so that it willpass a No. 14(1.40 micrometer) sieve and the cutting shall be continued until the entire sample passes through the sieve. 6 METHOD A 6.1 Outline of the Method 6.1.1 A weighed test portion of the rubber is extracted with ethanol toluene azeotrope solvent in a suitable apparatus (see Fig. 1 to 3). The solvent is distilled off and the residue is dried and weighed. 6.1.2Take duplicate test portions from the sample prepared in accordance with4.7. Take a test portion of about 3 g to 5 g and weigh it to the nearest 0.1 mg (mass M,). 6.13 Dry the chosen flask in the oven at 100 A 2W. Remove the flask from the oven and allow it to cool to room temperature in a desiccator, weigh to the nearest 0.1 mg (massMJ. 6.1.4 Roll the weighed test portion in filter paper or nylon filter cloth to form a loose roll from which the rubber cannot fall and so that no part of the rubber is anywhere in contact with arty other part of the rubber. If the test portion is in the form of small pieces, make a loose pocket of pieces in filter paper or nylon filter paper or nylon filter cloth. Fasten each test packet with clean wire. Place the packet in the appropriate extraction apparatus (see Fig. 1 to 3). Sufficient appropriate solvent to till the extraction cup two or three times and pour into the extraction flask adjust the heating rate so that the quantity of distilled solvent fills the extraction cap 10to 20 times per hour and extract for 16 ~0.5 h. 6.1.5 At the end of the heating period, turn off the heating device, allow the apparatus to cool, remove the extmctor or siphon cup and discard the rubber test portion unless it is required for further testing. 6.1.6 Dry the flask and contents for 2 h at 100~2W in the oven and, at the end of this time, remove the flask from the oven, cool in a desiccator and weigh to the nearest 0.1 mg (mass M3). 6.1.7 Can-ya blank through the entire procedure, using the same type of apparatus and quantity of solvent as for the test portion, but omitting the test portion, (Increase in mass,M,). 3 6.2 Calculation The solvent extractable material expressed as a percentage by mass, is given by the formula: M3­ MZ­ M4 M, where M, = mass, in grams of the test portion (see 6.1.2); Mz = the mass in grams, of the empty receiver flask (see 6.1.3); M3 = the mass, in grams of the receiver flask plus the extract after drying (see 6.1.6); and M, = increase in mass, in grams, of a receiver flask during the blank test (see 6.1.7). 63 Report 63.1 The report shall include the following: a) Proper identification of sample and reference standard; b) Sample preparation; c) Type of extraction apparatus; and d) Result obtained.
NOTE -- The results obtained may be different deprding on the method of sample preparation.

x 100

7 METHOD B " /.1 Cut test portions from sample prepared as in 4.8 weighing between 90 mg and 110 mg nearest to 0.01 mg. Take 4 to 6 test portions (mass M,). 7.2 Assemble the extraction apparatus (see Fig. 1 to 3) but cannot only the condenser to the flask No. Soxhlet, extractor cup or siphon cup is necessary - only the receiving flask and the condenser. `l%etest portion is placed directly in the solvent. Alternatively, any arrangement for boiling solvent and test portions can be used, for example a beaker covered with a watch glass, a beaker covered with another beaker containing cold water, etc. The solvent volume shall be held constant and may be replenished with fresh solvent should evaporation wcur. 73 Add about 25 ml of solvent for each test portion. Use a maximum of six test portions in a 250 ml receiver flask and four test portions in a 150 ml flask. Reflux for 6omin. 7.4 At the end of the heating period, turn off the heating &vice, allow the apparatus to cool, then remove the receiver flask from the condenser. Pour the contents of the flask into a clean 150 micrometer sieve to recover the extracted test pieces. Discard the solvent in an appropriate manner.

ISl1720(Part6)

:2001 Mz = mass, in grams, of the test portion after extraction (see 7.6). 7.8 Test Result A test result is the average of two determinations. 7.9 Test Report The test report shall include the following: a) a reference to this standard; b) full identification of the rubber tested; c) the method of sample preparation; d) whether method A or method B was used; e) which solvent was used; f) which apparatus was used for extraction; and g) the mean of the two determinations.

7.5 Gently bolt the extracted test portions between absorbent tissue to remove excess solvent and dry them separately at 100t 20Cfor 30 min or until the mass does not change by more than ~ 0.1 mg over a period of 10 min. 7.6 Cool the test portions for about 10 min in a desiccator and weigh each to the nearest 0.1 mg (massM,). 7.7 Calculation The solvent-extractable material, expressed as a percentage by mass, is given by formula

where Ml = mass, in grams, of the test portion before extraction (see 7.1); and

ISl1720(Part6)

:2001

ANNEX A
(Foreword) COMMllTEE COMPOSITION
!

Rubber Sectional Committee, PCD 14
Organization Representative(s) DR S. N. CHAKRAVARTV (Chairman) SW C. T. PAE SW R. V.GANDHI (Alternate) SHRt MANU M.PATSL SHrrtS. C. M.urY (Alternate)

Polym Consultants, New Delhi All In&laRubber Industries Association, Mumbai

AparLtd, Mumbai
Apollo Tyres Ltd, Kerala Association of Pl@ters of

Kerala,Cochh!

SHRt M. P. KANJOLtA (Alternate) SW T. D. VARKSV Smu A. JACOB
(Alternate) Sti K.J. JosePH

Automotive Tyre Manufacturers Association, New Delhi Bata India Ltd, Kblkata Bayer (India) Ltd, Mumbai Bids Tyres, Batasore CEAT ~res Ltd, Mumbai Cosmos India Rubber Worka Pvt Ltd, Mumbai Directorate General of Supplies & D@msals (DGS&D), New Delhi Dunlop lndia Ltd, Kolkata Escon Consultants Pvt Ltd, Kolkata Gujarat Reclaim & Rubber Products Ltd, Ankleshwar Hindustan Latex Ltd, Thiruvanarrthapuram, Kerala Indian Petrochemicals Corporation Ltd, Vadodara ICI Ltd, Chemicai Division, Kolkata J.K. Industries, Rajasthan Ministry of Dcfence (DGQA), New Delhl Ministry of Defence (R&D), Karrpur MRF Ltd, Chennai Mudi Rubher Ltd, Modipursm National Test House, Kolkata The Padinjarekara Agencies Ltd, Kottayam The Plantation Corporation of Kerala Ltd, Kottayam Phoenix Yule Ltd, Kolkata The Rubber Board, Kottayam Synthetics and Chemicals Ltd, Mumbai Tyre Corporation of India, Kolkata Thirumbadi Rubber Co Ltd, Coimbatore

SHRt P.K. Mcm.mm (Alternate) SHru THOMAS FALCD SHtU B. M.CHAODHURI SHIU S. M. MnRA (Alternate) SHru P.K. CHATIMUEE SHRI D. P.MUKHERJES
(Alternate) SHIU A,.uT CHOUDHURY

SHtU A.R.VARADARAJAN
(Alternate) SHRI S.V.HAJARNIS
SHIUPULIN L. KtNARNVMA sH5t A. K. SEHOAL

SHruSUNOSR 1A (Alternate) Stuu K. S. LONGANATHAN SHruD. P. Smw (Alternate) DR D. BANSIUSS CHAUDHURY (Alternate) SHRIB. K. SEN MEHUL PAm SHRI SHRt RAJENDRA V.GANDHI (Aftemate) SHRIJ. .%fAYAOASAN SHIU S. R.PANICKSR (Alternate) SHRI A.K.BASU % c. ~ Vm~A~ DR R.MUKHOPAOHVAY (Alternate) SHIU A,K.GAUSA Lr-COLJ. S. DUGOAL (Alternate) SHtU RAM CHANDRA Drr R. K. SmGH DR D. K. SMIJA(Alternate) George !$HIu ZACH W %U G. C. UPADHVAY SHiU K. K. AWASTHt (Alternate) SHRI D. N. RcrY (Alternate) DR I. N. MUKHERJEE
% f$ATIWt ABRAt'L4M

SHRI N. MDHANAKUMAR (Alternate) DR N. T. THOMAS sHRt T. K. hhGUZRJSE
DR A. GUHA (Alternate)

DRM. G. KUMARA~ SHRI M. SONNY SsaAsmN (Alremate) DR R. N. MSHRCrMA DR VFD PARKASH (Alternate) SHRI P. B. KONAR SHruK. P. KRtSHNAKUMAR

(Continued on page 6)

5

IS 11720(Part 6) :2001
(Continued from page 5)

Organization

The Travancore Rubber-& Tea Co Ltd, Trivandrum United Planters Association of Southern India, Coonoor

Representative(s) SHRtS. R. SARMA SHRtP. S. GOPtNATHAN (Alternate) SsuuK. JACOB THOMAS SHFUK. KANNAN (Alternate)

BIS Directorate General

ANIAN KAR,

Dkector& Head(pCD) [Representing DirectorGeneral(Ex-ofjicio)]

Member-Secretary R. P. MISHRA SHSU

Joint Director (pCD), BIS

Method of Testing Subcommittee, PCD 14:1
J. K. Industries Ltd, Rajasthan
DR R. MUKHOPAOHYAY (Convener) SHRt A. S. DEURI(Alternate I) SHtUS. DASOUFTA (Alternate II) SHRtMANUM. PATEL SHRtS. C. MAm (Alternate) B.M. CILWOHUSU SHSU SHRtHRZWttKESH CHAKRABORW (Alternate) SHRI P. K. CHATIEIUEE SHSU D. J. BHARUCHA (Alternate) SHRtA. ~A DR G. M. SrNHA ROY(Alternate) SHIUB. D. DUBEY SHst P. F. MILLER (Alternate) sHtUA. SUrCAR (Alternate) SHtUV. S. JAYARAM SHRt R. M. PANOIA DR B. SURYANABAYANAN (Alternate) SHRIC. M. GEOROE DR ANmK. BHOWMtCK (Alternate) DR D. K. TRIPATHV D. L. VYAS !+HtU SHtUN. K. GANOOPAOHYAY (Alternate) SHRtB. S. AOAFTA

Apar Ltd, Mumbai Bata India Ltd, Kolkata Bayer (India) Ltd, Mumbai Birla Tyres, Balasore Directorate General of Supplies & D@rosafs, New Delhi Dunlop India Ltd, Kolkata Herdillia Unimers Ltd, Mumbai Harrison Malayalam Limited Cochln, Kerala HT, Kharagpur Indian Petrochemicals Corpn Ltd, Vadodara Karnataka Forest Development Corporation, Bangalore Lathia Rubber Mfg Co Pvt Ltd, Mumbai Ministry of Defence (DGQA), New Delhi MRF Ltd, Chennai Modi Rubber Ltd, Modipuram National Organic Chemical Industries Ltd, Thaoe Padinjarekara Agencies Ltd. Kottayam Phoenix Yule Ltd, Kolkata The Rubber Board, Kottayam Synthetics and Chemicals Ltd, Mumbai The Thirumbadi Rubber Co Ltd, Coimbatore

, (AUemate) SHSU Y. S. LATHSA A. K. BmYOPAOHAYA SHRI SrsiaT. K. MnRA (Alternate) SSSRSA. CksntosJoHN .SHRSS. L.SHARMA
., SHSU c. s. INAMOAR SHRI D. S. DaaAI(Alternate)
ABR4HAM %tSlSATSBH Smu T. K. MUKHERJSE DRA. GUHA (Alternate) ~M. G.Kuw SPBAamAN (Alternate) SHIU M. SUNNY DR R. N. MEHROmtA DR S. K. CHAKRABORTV (Alternate) SHRIK. P. KSUSHNAKUMAR MENON SHRSC.HAMOOS

SrssuS. V.LAIHtA

6

Bureau of Indian

Standards

B] S is a statutory institution established under the Bureau of Zndian Standards Act,. 1986 to promote harmonious development of the activities of stardardization, marking and quality certification of goods and attending to connected matters in the coun@y. Copyright BI S has the copyright of all its pu~lications. No part of these publications may be reproduced in any form without the prior permission in writing of BIS. This does not preclude the free use, in the course of implementing the standard, of necessary details, such as symbols and sizes, type or grade designations. Enquiries relating to copyright be addressed to the Director (Publication), BIS. Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed periodically; a standard along with amendments is reaffirmed when such review indicates that no changes are needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of `B] S Handbook' and' Standards: Monthly Additions'. This Indian Standard has been developed from Dot: No. PCD 14( 1872). Amendments Issued Since Publication Amend No. Date of Issue Text Affected

BUREAU OF INDIAN STANDARDS Headquarters: ManakBhavan,913ahadur Shah Zafar Marg, New Delhi 110002 Telephones: 3230131,3233375,3239402 Regional Offices: Central Eastern Northern Southern Western Branches : Manak Bhavan, 9 Bahadur Shah Zafar Marg NEW DELHI 110002 : 1/14 C.I.T. Scheme VII M, V.I.P. Road, Kankurgachi CALCUTTA 700054 : SCO 335-336, Sector 34-A, CHANDIGARH 160022 Telegrams: Manaksanstha (Common to all offices) Telephone 3237617,3233841 3378499,3378561 { 3378626,3379120 603843 { 602025 2541216,2541442 { 2542519,2541315 8329295,8327858 { 8327891,8327892

: C.I.T. Campus, IV Cross Road, CHENNAI 600113 : Manakalaya, E9 MIDC, Marol, Andheri (East) MUMBAI 400093 : AHMEDABAD. BANGALORE. BHOPAL. BHUBANESHWAR. COIMBATORE. FARIDABAD. GHAZIABAD. GUWAHATI. HYDERABAD. JAIPUR. KANPUR. LUCKNOW. NAGPUR. NALAGARH, PATNA. PUNE. RAJKOT. THIRUVANANTHAPURAM.

.
Printed at Simco Printing Press, Delhi